CN114361402B - MXene-based modified layer modified dendrite-free lithium metal anode, preparation method thereof and lithium metal battery - Google Patents
MXene-based modified layer modified dendrite-free lithium metal anode, preparation method thereof and lithium metal battery Download PDFInfo
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Abstract
The invention discloses a dendrite-free lithium metal anode modified by an MXene-based modification layer, a preparation method thereof and a lithium metal battery. The method comprises the steps of: providing a monomer solution, wherein the monomer is a cyclic ether; dispersing MXene in the monomer solution to obtain a suspension; adding an initiator to the suspension; coating the suspension containing the initiator on the surface of the lithium metal negative electrode, and carrying out in-situ polymerization reaction to obtain the MXene/polymer modified lithium metal negative electrode. According to the invention, the cyclic ether is used as a polymer monomer, MXene is used as an embedded modifier, the cyclic ether is subjected to ring opening and intermolecular condensation reaction under the action of an initiator, and finally, a MXene/polymer modification layer is formed on the surface of the lithium metal negative electrode in situ, so that the limitation that dendrite growth of the lithium metal negative electrode is difficult to control is overcome, and interface contact of a lithium metal battery is optimized.
Description
Technical Field
The invention relates to the technical field of lithium metal batteries, in particular to a dendrite-free lithium metal negative electrode modified by an MXene/polymer modification layer, a preparation method thereof and a lithium metal battery.
Background
With the rapid development of electric vehicles and microelectronic technologies, advanced energy storage technologies are continually being explored. Lithium metal batteries are considered to be the most potential high energy density batteries in the next generation of energy storage devices because lithium metal anodes have a very high theoretical capacity (3860 mAh-g -1 ) And a very low redox potential (-3.04V vs. standard hydrogen electrode).
Despite these advantages, practical applications of lithium metal batteries still face a number of troublesome problems including side reactions of lithium metal with electrolyte, growth of lithium dendrites, and volume expansion. The nature of these problems is that unstable SEI (solid electrolyte interphase) films lead to uneven diffusion and deposition of Li. To address these issues, various strategies have been reported, such as modifying separators, constructing three-dimensional current collectors, introducing artificial SEI, adding functional electrolyte additives. Despite some breakthroughs in the nucleation and growth of uniform lithium, there are still significant challenges in developing a simple and effective method to solve the above problems.
Constructing a stable artificial SEI film is a more efficient method to depassivate lithium metal surfaces than electrochemically generated SEI films. Inorganic materials are widely used as protective layers for lithium metal anodes due to their high mechanical strength, e.g. Li 3 PO 3 、LiAlO x 、Li 3 N. However, inorganic materials are fragile and have poor flexibility, and in lithium metal batteries, volume expansion of lithium metal cathodes during cycling cannot be accommodated, resulting in rupture of the SEI film.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the defects in the prior art, the invention aims to provide an MXene/polymer modification layer modified dendrite-free lithium metal negative electrode, a preparation method thereof and a lithium metal battery, and aims to solve the problems that an SEI film constructed by the existing inorganic material cannot adapt to volume expansion of the lithium metal negative electrode in a circulating process, so that the SEI film is broken and the lithium metal negative electrode cannot be effectively protected.
The technical scheme of the invention is as follows:
a preparation method of a lithium metal anode modified by an MXene/polymer modification layer comprises the following steps:
providing a monomer solution, wherein the monomer is a cyclic ether;
dispersing MXene in the monomer solution to obtain a suspension;
adding an initiator to the suspension;
coating the suspension containing the initiator on the surface of the lithium metal negative electrode, and carrying out in-situ polymerization reaction to obtain the MXene/polymer modified lithium metal negative electrode.
Optionally, the cyclic ether is at least one of ethylene oxide, propylene oxide, ring Ding Ermi, 1, 3-Dioxan (DOL), epoxybutadiene, 1, 3-dioxan.
Optionally, the monomer solution is prepared by dissolving a monomer in an organic solvent, wherein the volume ratio of the monomer to the organic solvent is 1:0.5-2.5, and the organic solvent is at least one of ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene carbonate, diethyl carbonate and propylene carbonate.
Optionally, the MXene is Ta 2 C，Ti 2 C，Nb 2 C，V 2 C，Cr 2 C，Mo 3 C 2 ，Ti 3 C 2 At least one of them.
Optionally, the MXene comprises 2 to 10wt.% of the monomer solution.
Optionally, the initiator is at least one of azodiisobutyronitrile, azodiisoheptonitrile, lithium hexafluorophosphate, aluminum triflate, aluminum dichloride and diethyl aluminum chloride.
Optionally, the in-situ polymerization reaction time is 1-8 hours.
Optionally, the temperature of the in-situ polymerization reaction is 25-80 ℃.
Optionally, the thickness of the MXene/polymer finishing layer is 5-10 μm.
The MXene/polymer modified lithium metal negative electrode is prepared by the preparation method of the MXene/polymer modified lithium metal negative electrode.
A lithium metal battery comprises a lithium metal anode modified by an MXene/polymer modification layer.
The beneficial effects are that: according to the invention, the cyclic ether is used as a polymer monomer, MXene is used as an embedded modifier, the cyclic ether is subjected to ring opening and intermolecular condensation reaction under the action of an initiator, and finally a stable MXene/polymer modification layer is formed on the surface of the lithium metal negative electrode in situ. The MXene/polymer modification layer can effectively passivate the surface of lithium metal and inhibit the growth of lithium dendrites, overcomes the limitation that the dendrite growth of a lithium metal cathode is difficult to control, and optimizes the interface contact of a lithium metal battery.
Compared with the SEI film constructed by the existing inorganic material, the MXene/polymer modification layer prepared by the invention has the following advantages as SEI film: on the one hand, the polymer formed by in-situ polymerization of the cyclic ether monomer shows excellent lithium ion transmission capability due to the linear chain structure rich in ether bonds. The flexible polymer not only can provide good interface contact and reduce interface impedance, but also can adapt to the volume expansion of the lithium metal anode in the charge and discharge process and prolong the cycle life of the SEI film. On the other hand, in the monomer in-situ polymerization process, the MXene is gradually, uniformly and tightly connected on the surface of the lithium metal negative electrode by a polymer, and the MXene has high lithium affinity and low lithium nucleation energy barrier, so that the surface of the lithium metal negative electrode modified by the MXene/polymer modification layer can also form an electric field with uniform distribution in the charge and discharge process, thereby inhibiting the growth of lithium dendrites and inducing uniform deposition of lithium.
Drawings
FIG. 1 is a view of an MXene scanning electron microscope prepared by the method of example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of the surface of the lithium metal negative electrode prepared by the preparation method of the embodiment 1.
Fig. 3 is a graph showing the voltage versus time of a solid-state lithium metal symmetrical battery prepared by the preparation method of example 1 of the present invention.
FIG. 4 shows a solid LiFePO obtained by the method of producing example 1 according to the present invention 4 Specific discharge capacity versus cycle number of half cells.
Detailed Description
The invention provides an MXene/polymer modified dendrite-free lithium metal anode, a preparation method thereof and a lithium metal battery, and the invention is further described in detail below in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to obtain a lithium metal negative electrode with high safety characteristic and long cycle life, it is important to construct a stable SEI film on the surface of the lithium metal negative electrode to passivate the surface of the lithium metal and inhibit the growth of lithium dendrite; in order to fully satisfy the gap between laboratory scale and practical commercial application scale, a preparation method of a dendrite-free lithium metal anode which is simple to operate, safe and effective needs to be explored.
Based on the above, the embodiment of the invention provides a preparation method of a lithium metal anode modified by an MXene/polymer modification layer, which comprises the following steps:
s1, providing a monomer solution, wherein the monomer is cyclic ether;
s2, dispersing MXene in the monomer solution to obtain a suspension;
s3, adding an initiator into the suspension;
and S4, coating the suspension containing the initiator on the surface of the lithium metal negative electrode, and carrying out in-situ polymerization reaction to obtain the MXene/polymer modified lithium metal negative electrode.
In the embodiment, MXene is added into a monomer solution, cyclic ether is used as a polymer monomer, and then a polycondensation initiator is added to initiate ring opening and intermolecular condensation reaction of the cyclic ether monomer, so that a stable MXene/polymer modification layer is formed on the surface of lithium metal in situ. The modified lithium metal anode has a uniform, compact and smooth surface. The MXene/polymer modification layer can effectively passivate the surface of lithium metal and inhibit the growth of lithium dendrites, solves the problem of dendrite growth of a lithium metal negative electrode, and optimizes the interface contact of a lithium metal battery. The MXene/polymer modified layer modified dendrite-free lithium metal anode prepared by the embodiment can be applied to high-energy density solid-state lithium metal batteries.
In addition, the preparation method of the dendrite-free lithium metal anode modified by the MXene/polymer modification layer is simple to operate, has no potential safety hazard, is suitable for large-scale industrial production, and has universality.
The preparation method can be used for coating a layer of uniform and compact SEI film on the surface of the lithium metal negative electrode in situ, and simultaneously, the thickness and the size of the SEI film can be controlled according to the volume of the monomer solution coated on the surface of the lithium metal negative electrode. Further, the SEI film prepared in this embodiment may have a thickness of 5 to 10 μm. Experiments show that the SEI film in the thickness range has smooth and compact surface, and no redundant monomer solution overflows the boundary of the lithium metal anode in the preparation process, so that the thickness of the SEI film can be accurately controlled.
In step S1, in one embodiment, the cyclic ether is at least one of ethylene oxide, propylene oxide, ring Ding Ermi, 1, 3-Dioxan (DOL), epoxybutadiene, 1, 3-dioxan.
In one embodiment, the monomer solution is prepared by dissolving a monomer in an organic solvent, wherein the volume ratio of the monomer to the organic solvent is 1:0.5-2.5, and the organic solvent is at least one of ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene carbonate, diethyl carbonate and propylene carbonate.
In one embodiment, step S2 specifically includes: the MXene was uniformly dispersed in the monomer solution, and subjected to ultrasonic treatment (about 30 minutes of ultrasonic treatment) to prepare the suspension. By adopting the preparation method, the embodiment can prevent the agglomeration phenomenon of the MXene in the polymerization process, thereby realizing the preparation of the modified layer with the MXene uniformly dispersed.
The MXene of this example has an accordion-like layered structure and can be prepared by a green molten salt etching method. In one embodiment, the MXene is Ta 2 C，Ti 2 C，Nb 2 C，V 2 C，Cr 2 C，Mo 3 C 2 ，Ti 3 C 2 At least one of them.
In one embodiment, the MXene comprises 2 to 10wt.% of the monomer solution. Experiments have shown that the content of MXene in the monomer solution is not too high, otherwise it is disadvantageous to obtain a highly dispersed suspension.
Step S3 is to add an initiator to the suspension that initiates the polycondensation reaction of the cyclic ether monomer molecules. In one embodiment, the initiator is azobisisobutyronitrile, azobisisoheptonitrile, lithium hexafluorophosphate (LiPF) 6 ) At least one of aluminum triflate, aluminum dichloride and diethyl aluminum chloride.
In one embodiment, the initiator is present in the monomer solution at a concentration of 0.5 to 2 mol.L -1 。
In step S4, in one embodiment, the volume of the suspension containing the initiator is coated on the surface of the lithium metal negative electrode to be 10 to 100 μl, so as to ensure that an MXene/polymer modified layer with a suitable thickness is formed on the surface of the lithium metal negative electrode.
In one embodiment, the in situ polymerization is for a period of time ranging from 1 to 8 hours.
In one embodiment, the in situ polymerization reaction temperature is 25 to 80 ℃. In-situ polymerization in this example can be carried out at room temperature.
The embodiment of the invention provides a lithium metal negative electrode modified by an MXene/polymer modification layer, wherein the lithium metal negative electrode modified by the MXene/polymer modification layer is prepared by the preparation method of the lithium metal negative electrode modified by the MXene/polymer modification layer.
The embodiment of the invention provides a lithium metal battery, which comprises the MXene/polymer modified layer modified lithium metal anode.
The invention will be further illustrated with reference to specific examples.
Example 1
1. MXene (Ti) was prepared according to the following procedure 3 C 2 )：
Will be 0.5g Ti 3 AlC 2 Powder and 1.03g CuCl 2 The powders were mixed (molar ratio 1:3) and milled for 10min. Then 0.3g NaCl and 0.38g KCl were added to the above mixture and the mixture was further milled for 10min. Subsequently, the mixture was uniformly dispersed in a corundum crucible, and high-temperature sintering was performed under an argon atmosphere using a tube furnace at 4℃min -1 The mixture was heated to 700 c and held for 24 hours. And then washed with deionized water to remove the remaining salt, resulting in a MXene/copper mixed powder. Then use 0.1 mol.L -1 The MXene/copper mixed powder was washed with ammonium persulfate solution to remove the remaining copper particles and further washed 5 times with deionized water and ethanol and filtered with a microfiltration membrane (polyvinylidene fluoride, 0.45 μm). Finally, vacuum drying is carried out at 60 ℃ for 24 hours. The resulting MXene powder was a layered two-dimensional material as shown in fig. 1.
2. The MXene/polymer modification layer modified dendrite-free lithium metal anode was prepared as follows:
MXene powder (5 wt.%, relative)At the weight of DOL/DME) was dispersed in a monomer solution of 0.5ml DOL and 0.5ml DME, and a homogeneous suspension was obtained after 30min of sonication. 0.1419g of LiPF are then added 6 Initiator and stirred for 5min. Finally, 100 mu L of the obtained suspension containing the initiator is taken out and immediately coated on the surface of the lithium metal negative electrode, and in-situ polymerization reaction is carried out for 8 hours, so that the MXene/polymer modified lithium metal negative electrode is obtained. The surface of the obtained lithium metal anode is uniform, smooth and compact, as shown in figure 2.
3. The solid-state lithium metal battery is prepared according to the following steps:
1.6g of polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) was dissolved in 5mL of N, N-Dimethylformamide (DMF) and stirred at 40℃for 30min. After the solution was completely transparent, 0.8g of Li was added 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 (LATP) particles, sonicated for 30min, and magnetically stirred for 12h to give a uniform dispersion. Subsequently, 3.2g of lithium bis (trifluoromethanesulfonyl imide) (LiTFSI) was added to the dispersion, and after magnetically stirring for 12 hours, the resulting white dispersion was cast into a glass petri dish, immediately transferred to a vacuum oven at 80℃and dried for 24 hours. Finally, the prepared PVDF-HFP/LATP composite electrolyte membrane was cut into disks having a diameter of 17mm, and then the electrolyte was stored in an inert atmosphere for the next use.
The lithium metal battery is assembled in an inert atmosphere. LiFePO is used for anode 4 The positive electrode or lithium metal, the negative electrode was modified with the MXene/polymer modified layer prepared in step 2, and the electrolyte was PVDF-HFP/LATP composite electrolyte membrane (diameter=17 mm, thickness=80 μm).
Wherein, liFePO 4 Positive electrode (3.1 mg cm) -2 ) By mixing 80wt.% LiFePO in N-methyl-2-pyrrolidone (NMP) 4 Powder, 10wt.% conductive carbon black and 10wt.% polyvinylidene fluoride (PVDF), magnetically stirring for 8 hours, coating the obtained slurry on aluminum foil by a scraper, drying for 12 hours at 70 ℃, and then drying for 12 hours at 80 ℃ in vacuum to obtain a battery anode, which can be used for lithium ion batteries.
When applied to lithium ion batteries, in symmetrical lithium metal batteries, the lithium ion batteries are respectively provided with a lithium ion battery capacity of 0.5mAh cm -2 Capacity and 0.2 mA.cm -2 The current was cycled steadily for 1000h and the overpotential was kept at 50mV. In LiFePO 4 In the battery, after the battery is stably circulated for 900 circles under the current of 1C, the capacity is kept at 130.1 mAh.g -1 The capacity retention was 91.4%. As shown in fig. 3 and 4. Wherein 0% MXene refers to a lithium metal negative electrode prepared without adding MXene powder to the monomer solution in step 2, 5% MXene refers to a lithium metal negative electrode prepared with adding 5wt.% MXene powder to the monomer solution in step 2, and prine Li refers to a lithium metal negative electrode without any treatment.
In summary, the invention provides a dendritic-free lithium metal anode modified by an MXene/polymer modification layer, a preparation method thereof and a lithium metal battery. The modified lithium metal anode has a uniform, compact and smooth surface. The MXene/polymer modification layer solves the dendrite growth problem of the lithium metal negative electrode and optimizes the interface contact of the lithium metal battery. The MXene/polymer modified layer modified dendrite-free lithium metal anode prepared by the invention can be applied to high-energy density solid lithium metal batteries. In addition, the preparation method of the dendritic crystal-free lithium metal anode modified by the MXene/polymer modification layer is simple to operate and free of potential safety hazards, is suitable for large-scale industrial production, and has universality.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (10)
1. The preparation method of the MXene/polymer modified lithium metal anode is characterized by comprising the following steps:
providing a monomer solution, wherein the monomer is a cyclic ether;
dispersing MXene in the monomer solution to obtain a suspension;
adding an initiator to the suspension;
coating the suspension containing the initiator on the surface of the lithium metal negative electrode, and carrying out in-situ polymerization reaction to obtain the MXene/polymer modified lithium metal negative electrode.
2. The method for preparing a lithium metal anode modified by a MXene/polymer modification layer according to claim 1, wherein the cyclic ether is at least one of ethylene oxide, propylene oxide, ring Ding Ermi, 1, 3-dioxapentacyclic, epoxybutadiene, 1, 3-dioxanic.
3. The method for preparing the MXene/polymer modified lithium metal anode according to claim 1, wherein the monomer solution is prepared by dissolving a monomer in an organic solvent, the volume ratio of the monomer to the organic solvent is 1:0.5-2.5, and the organic solvent is at least one of ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene carbonate, diethyl carbonate and propylene carbonate.
4. The method for preparing a modified lithium metal anode of MXene/polymer modification layer according to claim 1, wherein the MXene is Ta 2 C，Ti 2 C，Nb 2 C，V 2 C，Cr 2 C，Mo 3 C 2 ，Ti 3 C 2 At least one of them.
5. The method for producing a modified lithium metal anode of an MXene/polymer modification layer according to claim 1, characterized in that the MXene accounts for 2 to 10wt.% of the monomer solution.
6. The method for preparing a lithium metal anode modified by a MXene/polymer modification layer according to claim 1, wherein the initiator is at least one of azodiisobutyronitrile, azodiisoheptonitrile, lithium hexafluorophosphate, aluminum triflate, aluminum dichloride and diethyl aluminum chloride.
7. The method for preparing a modified lithium metal anode of an MXene/polymer modification layer according to claim 1, characterized in that the time of the in situ polymerization is 1 to 8 hours, and the temperature of the in situ polymerization is 25 to 80 ℃.
8. The method for producing a modified-MXene/polymer modified-layer lithium metal anode according to claim 1, wherein the thickness of the MXene/polymer modified layer is 5-10 μm.
9. An MXene/polymer modified lithium metal negative electrode characterized by being prepared by the method for preparing an MXene/polymer modified lithium metal negative electrode according to any one of claims 1 to 8.
10. A lithium metal battery comprising the MXene/polymer modified lithium metal negative electrode of claim 9.
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| Excellent electrolyte-electrode interface stability enabled by inhibition of anion mobility in hybrid gel polymer electrolyte based Li-O-2 batteries;Yang, TS等;《JOURNAL OF MEMBRANE SCIENCE 》;118051 * |
| Polypyrrole-Encapsulated Polyoxomolybdate Decorated MXene As a Functional 2D/3D Nanohybrid for a Robust and High Performance Li-Ion Battery;Mahajan, M等;《ACS APPLIED ENERGY MATERIALS》;4541-4550 * |
| 半结晶、耐溶剂膜材料在膜萃取卤水提锂中的应用;张春风等;《膜科学与技术》;171-178 * |
| 离子电导率增强的聚合物电解质的制备及其在锂氧电池中的应用;杨庭帅;《中国优秀硕士学位论文全文数据库》;B016-178 * |
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| CN114361402A (en) | 2022-04-15 |
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